CN101485736A - Medicament composition with stone-eliminating and expelling functions and preparation method thereof - Google Patents
Medicament composition with stone-eliminating and expelling functions and preparation method thereof Download PDFInfo
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Abstract
The invention provides a medical composition with functions of dissolving and discharging stones, which is tablets prepared from Herba Lysimachiae, stir-fried cowherb seed, Common Knotgrass Herb, Corydalis tuber processed by vinegar, scalded Endothelium Corneum Gigeriae Galli, Salvia Miltrorrhiza, Radix Aucklandiae, fringed pink, Radix Cyathulae, Japanese Climbing Fern Spore, pharmaceutic adjuvants starch, magnesium stearate and sodium carboxymethyl starch which are taken as raw materials. A lubricant magnesium stearate is added by an equal quantity increasing method to improve particle fluidity and make particles pressed into the tablets; and a disintegrant sodium carboxymethyl starch is added by the equal quantity increasing method, so that the tablets can be disintegrated in 60 minutes to solve the difficult problem that the tables cannot be prepared and overcome the defect that the particles are easy to absorb damp. The preparation has the advantages of stability, safe administration, accurate dosage, controllable quality, reliable healing effect, high contents of effective ingredients, small administrative dosage, convenient administration, and is sugar-free to be suitable for more patients.
Description
Technical field
The present invention relates to a kind of pharmaceutical composition with fossil, calculus effect; The invention still further relates to this preparation of drug combination method, belong to the field of Chinese medicines.
Background technology
The logical granule of nephrolith is a kind of Chinese patent medicine of classics.It makes granule by Herba Lysimachiae, Semen Vaccariae (parched), Herba Polygoni Avicularis, Rhizoma Corydalis (processed with vinegar), boiling hot Endothelium Corneum Gigeriae Galli, Radix Salviae Miltiorrhizae, the Radix Aucklandiae, Herba Dianthi, Radix Achyranthis Bidentatae, Spora Lygodii ten flavor Chinese herbal medicine.The logical granule of this nephrolith has clearing away heat-damp and promoting diuresis, promoting blood circulation and stopping pain, and fossil, the urinary calculus removing effect is used for renal calculus, pyelolithiasis, the clinical treatment of diseases such as ureteral calculus.But said preparation is a granule, and dosage form is comparatively backward, and the granule dose is big, and taking needs boiled water to take after mixing it with water, and contains a large amount of sucrose and be not suitable for diabetic and take, and the easy moisture absorption of granule, is prone to caking phenomenon in the storage process.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, and a kind of pharmaceutical composition with fossil, calculus effect is provided.Another technical scheme of the present invention has provided this preparation of drug combination method.
A kind of pharmaceutical composition with fossil, calculus effect is characterized in that it is the tablet of being made by following weight percentages and pharmaceutic adjuvant,
Herbal raw material:
Herba Lysimachiae 15.5-17.5%, Semen Vaccariae (parched) 15.5-17.5%, Herba Polygoni Avicularis 9.5-11.5%, Rhizoma Corydalis (processed with vinegar) 4.5-5.5%, boiling hot Endothelium Corneum Gigeriae Galli 5.5-7.5%, Radix Salviae Miltiorrhizae 5.5-7.5%, Radix Aucklandiae 2.5-3.5%, Herba Dianthi 8-10%, Radix Achyranthis Bidentatae 4.5-5.5%, Spora Lygodii 5.5-7.5%;
Pharmaceutic adjuvant:
Filler 14-15% lubricant 0.01-0.15%, disintegrating agent 0.35-0.45%.
Further preferably, described filler is a starch; Lubricant is a magnesium stearate; Disintegrating agent is a carboxymethyl starch sodium.
Further preferably, it is the tablet of being made by following weight percentages and pharmaceutic adjuvant,
Herbal raw material:
Herba Lysimachiae 16.7% Semen Vaccariae (parched) 16.7% Herba Polygoni Avicularis 10.0%
Rhizoma Corydalis (processed with vinegar) 5.0% scalds Endothelium Corneum Gigeriae Galli 6.7% Radix Salviae Miltiorrhizae 6.7%
The Radix Aucklandiae 3.3% Herba Dianthi 8.4% Radix Achyranthis Bidentatae 5.0%
Spora Lygodii 6.7%
Pharmaceutic adjuvant:
Starch 14.1% magnesium stearate 0.1% carboxymethyl starch sodium 0.4%
Wherein, in the described tablet every contain Herba Lysimachiae, Herba Polygoni Avicularis with Quercetin (C
15O
10H
7) meter, must not be less than 0.10 milligram.
The present invention also provides a kind of method for preparing described pharmaceutical composition, wherein, in the described 10 flavor herbal raw materials, get Spora Lygodii, Semen Vaccariae and pack in the cloth bag, decoct with water secondary with eight flavors such as all the other Herba Lysimachiaes, 2.5 hours for the first time, 1.5 hours for the second time, collecting decoction filtered, decompression (75 ℃ ,-0.07Mpa) be concentrated into the extractum that relative density is 1.20～1.25 (75～80 ℃); Make adjuvant with starch, mixing is granulated, dry below 80 ℃; Granulate adds carboxymethyl starch sodium and magnesium stearate, mixing, and compacting is wrapped film-coat in flakes, promptly gets tablet.
Wherein, the consumption of described starch is that the extractum amount is in 1.8～2.1 times of dried cream; Further preferably, the consumption of described starch is that the extractum amount is in 1.85 times of dried cream.
Wherein, described method of granulating is for adopting boiling granulating machine fluidized granulating, and technical parameter is: feed liquor speed 50～55ml/min; Atomisation pressure 0.15Mpa; 55～60 ℃ of temperature of charge; 80～100 ℃ of inlet temperature; 60～65 ℃ of leaving air temps.The boiling granulating machine can be selected the granulator of plurality of specifications for use, as FL-120 type boiling granulating machine.
Wherein, the consumption of described carboxymethyl starch sodium is that the extractum amount is in dried cream 0.1%w/w; The consumption of described magnesium stearate is that the extractum amount is in dried cream 0.4%w/w.The adding method of described carboxymethyl starch sodium, magnesium stearate is the equivalent incremental method, adds carboxymethyl starch sodium earlier, adds magnesium stearate again.
The invention has the beneficial effects as follows: adopt the equivalent incremental method to add magnesium stearate lubricant, improve mobility of particle, granule can be suppressed in flakes; Adopt the equivalent incremental method to add disintegrating agent carboxymethyl base Starch Sodium and make the tablet can disintegrate in 60 minutes, solved the difficult problem that to make tablet, overcome the shortcoming that granule is easy to the moisture absorption.Medicinal tablet effective component content height of the present invention, taking dose be little, it is more convenient to take, be suitable for that the crowd is more extensive, outward appearance is all good.
Below the present invention is described in further detail by the specific embodiment, but do not limit the present invention, those skilled in the art can make various changes and distortion according to the present invention, only otherwise break away from spirit of the present invention, all should belong to the scope of claims of the present invention.
The specific embodiment
The preparation of embodiment 1 pharmaceutical composition tablet of the present invention
Herbal raw material (unit: gram):
Herba Lysimachiae 375g, Semen Vaccariae (stir-fry) 375g, Herba Polygoni Avicularis 225g, Rhizoma Corydalis (vinegar system) 112.5g, Endothelium Corneum Gigeriae Galli (scalding) 150g, Radix Salviae Miltiorrhizae 150g, Radix Aucklandiae 75g, Herba Dianthi 187.5g, Radix Achyranthis Bidentatae 112.5g, Spora Lygodii 150g.
Pharmaceutic adjuvant:
Starch 315g magnesium stearate 2.5g carboxymethyl starch sodium 10g
Its preparation method is, in the above 10 flavor Chinese herbal medicine, getting Spora Lygodii, Semen Vaccariae packs in the cloth bag, decoct with water secondary with eight flavors such as all the other Herba Lysimachiaes, 2.5 hours for the first time, 1.5 hours for the second time, collecting decoction, filter, decompression (75 ℃ ,-0.07Mpa) be concentrated into the extractum that relative density is 1.25 (75 ℃); Make adjuvant with starch, mixing is granulated, dry below 80 ℃; Granulate adds carboxymethyl starch sodium and magnesium stearate, and mixing is pressed into 1000, and the bag film-coat promptly gets medicinal tablet of the present invention.
The preparation of embodiment 2 pharmaceutical composition tablets of the present invention
Herbal raw material:
Herba Lysimachiae 16.7% Semen Vaccariae (parched) 16.7% Herba Polygoni Avicularis 10.0%
Rhizoma Corydalis (processed with vinegar) 5.0% scalds Endothelium Corneum Gigeriae Galli 6.7% Radix Salviae Miltiorrhizae 6.7%
The Radix Aucklandiae 3.3% Herba Dianthi 8.4% Radix Achyranthis Bidentatae 5.0%
Spora Lygodii 6.7%
Pharmaceutic adjuvant:
Starch 14.1% magnesium stearate 0.1% carboxymethyl starch sodium 0.4%
Its preparation method is, in the above 10 flavor Chinese herbal medicine, getting Spora Lygodii, Semen Vaccariae packs in the cloth bag, decoct with water secondary with eight flavors such as all the other Herba Lysimachiaes, 2.5 hours for the first time, 1.5 hours for the second time, collecting decoction, filter, decompression (75 ℃ ,-0.07Mpa) be concentrated into the extractum that relative density is 1.25 (75 ℃); Make adjuvant with starch, mixing is granulated, dry below 80 ℃; Granulate adds carboxymethyl starch sodium and magnesium stearate, mixing, and compacting is wrapped film-coat in flakes, promptly gets medicinal tablet of the present invention.
The preparation of embodiment 3 pharmaceutical composition tablets of the present invention
Herbal raw material:
Herba Lysimachiae 15.5% Semen Vaccariae (parched) 15.5% Herba Polygoni Avicularis 9.5%
Rhizoma Corydalis (processed with vinegar) 4.5% scalds Endothelium Corneum Gigeriae Galli 7.5% Radix Salviae Miltiorrhizae 7.5%
The Radix Aucklandiae 3.5% Herba Dianthi 10% Radix Achyranthis Bidentatae 4.5%
Spora Lygodii 7.5%
Pharmaceutic adjuvant:
Starch 14% magnesium stearate 0.15% carboxymethyl starch sodium 0.35%
Its preparation method is, in the above 10 flavor Chinese herbal medicine, getting Spora Lygodii, Semen Vaccariae packs in the cloth bag, decoct with water secondary with eight flavors such as all the other Herba Lysimachiaes, 2.5 hours for the first time, 1.5 hours for the second time, collecting decoction, filter, decompression (75 ℃ ,-0.07Mpa) be concentrated into the extractum that relative density is 1.22 (78 ℃); Make adjuvant with starch, mixing is granulated, dry below 80 ℃; Granulate adds carboxymethyl starch sodium and magnesium stearate, mixing, and compacting is wrapped film-coat in flakes, promptly gets medicinal tablet of the present invention.
The preparation of embodiment 4 pharmaceutical composition tablets of the present invention
Herbal raw material:
Herba Lysimachiae 17.5% Semen Vaccariae (parched) 17.5% Herba Polygoni Avicularis 11.5%
Rhizoma Corydalis (processed with vinegar) 5.5% scalds Endothelium Corneum Gigeriae Galli 5.5% Radix Salviae Miltiorrhizae 5.5%
The Radix Aucklandiae 2.5% Herba Dianthi 8% Radix Achyranthis Bidentatae 5.5%
Spora Lygodii 5.5%
Pharmaceutic adjuvant:
Starch 15% magnesium stearate 0.05% carboxymethyl starch sodium 0.45%
Its preparation method is, in the above 10 flavor Chinese herbal medicine, getting Spora Lygodii, Semen Vaccariae packs in the cloth bag, decoct with water secondary with eight flavors such as all the other Herba Lysimachiaes, 2.5 hours for the first time, 1.5 hours for the second time, collecting decoction, filter, decompression (75 ℃ ,-0.07Mpa) be concentrated into the extractum that relative density is 1.20 (80 ℃); Make adjuvant with starch, mixing is granulated, dry below 80 ℃; Granulate adds carboxymethyl starch sodium and magnesium stearate, mixing, and compacting is wrapped film-coat in flakes, promptly gets medicinal tablet of the present invention.
Embodiment 5 drug quality control methods of the present invention
(1) get 10 of this product, remove coating after, porphyrize adds ethanol 30ml, reflux 30 minutes is put coldly, filters the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, uses the chloroform extraction secondary, each 15ml, combined chloroform liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, and as need testing solution, other gets Endothelium Corneum Gigeriae Galli control medicinal material 2g, add ethanol 20ml, reflux 30 minutes is put coldly, filters, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethanol acetate-formic acid (3:3:0.5) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, put dry by the fire in the baking oven to the speckle colour developing clear.In the chromatograph for examination, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) get 6 of this product, remove coating after, porphyrize, add methanol 50ml, supersound process 15 minutes filters, filtrate evaporate to dryness, residue add water makes dissolving, adds strong ammonia solution and transfers to alkalescence, extract 3 times with the ether jolting, each 10ml divides and gets ether layer, ether solution evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Rhizoma Corydalis control medicinal material 0.5g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, with petroleum ether (60～90 ℃)-chloroform-methanol (10: 4: 0.5) is developing solvent, launch, take out, dry, iodine is smoked, puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
(3) get 6 of this product, remove coating after, porphyrize, add 70% ethanol 30ml, supersound process 15 minutes filters, evaporate to dryness in the filtrate water-bath, residue adding distil water 25ml makes dissolving, transfers pH to 2 with dilute hydrochloric acid, with ether 25ml extraction 2 times, divide and get ether layer, ether solution evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Radix Salviae Miltiorrhizae control medicinal material 0.5g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-acetone-formic acid (10: 4: 1.6) is developing solvent, launch, take out, dry, put in the ammonia steam smoked after, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
The test that the adjuvant of embodiment 6 pharmaceutical composition tablets of the present invention and adjuvant are selected
1, medicinal tablet medicinal material extract of the present invention, concentration technology
Adopt in the logical granule long-term production of nephrolith that decocting boils, concentrating under reduced pressure technology, process stabilizing, long-term clinical application proves: finished product application safety, determined curative effect.Medicine material extraction process of the present invention is: get the prescription medical material, Spora Lygodii, Semen Vaccariae are packed in the cloth bag, decoct with water secondary with eight flavors such as all the other Herba Lysimachiaes, add 8 times of water gagings for the first time, decoct 2.5 hours; For the second time double water gaging, decocted 1.5 hours, collecting decoction is crossed 200 mesh sieve fine straining after crossing 80 mesh sieve coarse filtration, reduce pressure (75 ℃ ,-0.07Mpa) be concentrated into the extractum that relative density is 1.20～1.25 (75～80 ℃).
2, medicinal tablet Study on Forming of the present invention
2.1 prescription design
Because of the logical granule prescription of former nephrolith usage and dosage is: oral, a daily dose primary crude drug 15.3g.Now make tablet, relate to the formulation usage and dosage, inevitable relevant with Chinese medical concrete amount and supplementary product consumption.One daily dose primary crude drug 15.3g, paste volume is 1.38g, and by taking every day 2 times, each 4, specification (plain sheet) is the 0.5g/ sheet, and then adjuvant need add 2.62g.According to last calculating, preparation prescription is:
Extract medical material 1912.5g (the logical granule of nephrolith has 3.75 times of sugared type recipe quantity), paste volume is about 172.5g, and (the logical granule medicinal material extract rate average out to of nephrolith in the long-term production: 9.02%), make 1000 altogether, adjuvant need add 327.5g.
Herba Lysimachiae 375g, Semen Vaccariae (stir-fry) 375g, Herba Polygoni Avicularis 225g, Rhizoma Corydalis (vinegar system) 112.5g, Endothelium Corneum Gigeriae Galli (scalding) 150g, Radix Salviae Miltiorrhizae 150g, Radix Aucklandiae 75g, Herba Dianthi 187.5g, Radix Achyranthis Bidentatae 112.5g, Spora Lygodii 150g
2.2 granulation supplementary product kind screening
The water extracted immersing paste should add a certain amount of adjuvant when granulating, and generally selects starch, dextrin, sucrose to get final product.Granulate so that the starch, dextrin, sucrose of 190% amount are manual respectively in the experiment, be placed in 75.28% the relative humidity (25 ℃) 72 hours.Investigate particulate hydroscopicity.The results are shown in Table 1
Table 1 supplementary product kind screening table
Add starch, dextrin, sucrose hydroscopicity basically identical as shown in Table 1 respectively,, select starch to get final product because starch is adjuvant commonly used.
2.3 supplementary product consumption screening
Granulate by adding starch in the experiment, investigate its hygroscopicity, the results are shown in Table 2 with method with the dried cream different proportion of theory.
The screening of table 2 starch consumption
It is better when the starch addition is in 1.8～2.1 times of dried cream of theory as seen from the above table.But the starch addition is many, and dose is just big, is advisable about 1.85 times (315g) that therefore definite starch addition is dried cream amount.
2.4 granulating process research
(1), method of granulating
Adopt FL-120 type boiling granulating machine boiling granulating, add recipe quantity starch and make bed material, taking liquid is done binding agent, spray into, and boiling granulating in fluid bed, promptly.
(2), the investigation of granulating process condition
The fluidized granulating important technological parameters is screened, and concrete outcome sees Table 3.
Table 3 fluidized granulating important technological parameters is investigated
The important technological parameters of fluidized granulating is as shown in Table 3: feed liquor speed 50～55ml/min; Atomisation pressure 0.15Mpa; 55～60 ℃ of temperature of charge; 80～100 ℃ of inlet temperature; 60～65 ℃ of leaving air temps.
2.5 practical physical property research
(1), character
Brown granular, bitter in the mouth is little puckery.
(2), bulk density
Take by weighing the qualified granule of constant weight, in the 10ml graduated cylinder of packing into, fall (controlled condition unanimity as far as possible) for several times, make the degree of tightness appropriateness, get bulk density divided by volume, the results are shown in Table 4 with weight with certain altitude.
Table 4 granulation mass density measurement result
(3), the mensuration of angle of repose
Get qualified granule and flow down and be cone shape, measure its angle of repose, the results are shown in Table 5 through funnel.
Table 5 granule angle of repose
(4), selection of lubricants
Last table shows, boiling granulating, and particle is more loose, and flowability is relatively poor a little, can't suppress qualified tablet, is improved so must make with lubricator.
Experiment by total method of mixing with lubricant: Pulvis Talci, magnesium stearate, the parallel adding experiment of micropowder silica gel granule, with total mix the machine mix homogeneously after, measure through draw samples, it is very big that same lubricant always mixes the back difference of flowability with granule.After adopting the equivalent incremental method to add lubricant, difference of flowability was then very little after same lubricant mixed with granule.
The screening of lubricant kind sees Table 6, adopts the equivalent incremental method to add its addition 0.5%.
The screening of table 6 lubricant
Select magnesium better relatively by table 6.Adopt the equivalent incremental method to add, its consumption screening sees Table 7.
Table 7 magnesium stearate consumption screening table
Therefore, it is better about 0.5% (2.5g) establishing the magnesium stearate consumption.
(5), the granule critical relative humidity is measured
Get 7 parts of qualified granules, every part of about 2g, the accurate title, decide, be placed on the exsiccator interior (the weighing bottle cap is opened) of the listed supersaturated solution that fills 7 kinds of different salt respectively of table 8, place weighing after 48 hours in 25 ℃ of constant incubators, calculate the moisture absorption percentage rate, it the results are shown in Table 9.
With the moisture absorption percentage rate is vertical coordinate, and relative humidity is the abscissa mapping, the results are shown in Figure 1.
The relative humidity of the supersaturated solution of table 8 variable concentrations sulphuric acid or different salt in the time of 25 ℃
Table 9 critical relative humidity determination data
Measurement result as seen, the granule critical relative humidity is 71%, has certain moisture, its production requirement can be satisfied in general tablet workshop.
2.6 tablet forming technique research
(1), the selection of disintegrating agent
A, with disintegrating agent, compressed tablets is disintegration: 66 minutes.Do not meet relevant laws and regulations tablet general rule requirements such as pharmacopeia, must be improved by experiment just and can make qualified tablet.
B, this product are full extractum sheet, and the experiment confirm disintegrate is slower, must be improved with disintegrating agent.
Experiment by total method of mixing with disintegrating agent: dry starch, carboxymethyl starch sodium, the parallel adding experiment of low substituted hydroxy cellulose granule, behind total mixed machine mix homogeneously, after the compacting in flakes, measure slice, thin piece disintegration through draw samples, the disintegration of tablet time limit that same disintegrating agent makes is widely different, has defective phenomenon.After adopting the equivalent incremental method to add disintegrating agent, compacting is in blocks, and the disintegration of tablet time limit difference that same disintegrating agent makes is very little, does not have defective phenomenon.
The screening of disintegrating agent kind sees Table 10, adopts the equivalent incremental method to add its addition 2%.
The screening of table 10 disintegrating agent
Select the carboxymethyl starch sodium disintegrating agent better relatively by table 10.Adopt the equivalent incremental method to add, its consumption screening sees Table 11.
Table 11 carboxymethyl starch sodium consumption screening table
Therefore, it is better about 2.0% (10g) establishing the carboxymethyl starch sodium consumption.
(2), the mode particular determination of the addition sequence of carboxymethyl starch sodium and magnesium stearate and adding.
Through The effects, the addition sequence of carboxymethyl starch sodium and magnesium stearate and the mode of adding have a significant effect to the preparation effect, therefore, the addition sequence of carboxymethyl starch sodium and magnesium stearate and the mode of adding are made particular determination.
The addition sequence of table 12 carboxymethyl starch sodium and magnesium stearate and the mode of adding are investigated experiment
Among the preparation technology of existing tablet, the addition sequence of disintegrating agent and flowable is little to the quality influence of tablet, does not do specific (special) requirements in the preparation process; Be surprised to find that by above-mentioned test the adding method of disintegrating agent of the present invention and flowable has determined to be pressed into the quality of tablet.Wherein, adopt the equivalent incremental method earlier with disintegrating agent, it is best to add the flowable mode again, the tablet best results of compacting.
(3), mixing uniformity is investigated
In order to guarantee the end product quality homogeneity, serve as to investigate index with quercetin content uniformity in the granule (sneaking into all adjuvants) for this reason, investigated three-dimensional mixer with the mixed mixing uniformity of granule, magnesium stearate and carboxymethyl starch sodium.
Test method: be divided into three layers of upper, middle and lowers after will mixing, every layer is selected two some sampling and measuring quercetin contents, calculates the RSD value of 6 points.
Content assaying method: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000).
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler, is mobile phase with methanol-0.2% phosphoric acid solution (55: 45), detects wavelength 370nm, and number of theoretical plate calculates with the Quercetin peak should be not less than 2500.
The preparation of reference substance solution: precision takes by weighing Quercetin reference substance 10.1mg, puts in the 50ml measuring bottle, with dissolve with methanol and be diluted to scale, shakes up; Get 1ml to 10ml measuring bottle, with dissolve with methanol and be diluted to scale, shake up, promptly get (containing Quercetin 0.0202mg among every 1ml).
The preparation of need testing solution: it is an amount of to get this product, and porphyrize is got the about 3g of fine powder, the accurate title, decide, and puts in the 100ml conical flask, adds methanol solution 30ml and hydrochloric acid 1ml, put in 85 ℃ of water-baths and refluxed 1 hour, be cooled to room temperature, change in the 50ml measuring bottle, be diluted to scale with methanol, shake up, the accurate 2ml that inhales is in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, centrifugal, cross microporous filter membrane (0.45um), get filtrate as need testing solution.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
The results are shown in Table 13:
The blended uniformity of table 13 granule is table as a result
Result of the test shows, RSD＜2%, and mix homogeneously, selected technology can be produced stay-in-grade finished product, and technology is rationally feasible.
(4), the selection of pellet moisture
The granule that makes tablet machine tabletting influences the pellet moisture that has of tablet quality, and the granule plasticity of the suitable moisture of water content is big, and the hardness of the tablet that is pressed into is better, and granule is too wet, and sticking then easily takes place.The pellet moisture screening sees Table 14.
The screening of table 14 pellet moisture
Pellet moisture should be controlled in 2%～5% better as shown in Table 14.Inner quality standard is decided to be: 2.5%～3.5%.
2.7 art for coating research
Because this product is full extractum sheet, the moisture absorption for improving plain tablet quality, is got coating so adopt easily.Film coating compare with sugar-coat have with short production cycle, consumption is few, sheet heavily increase little, clothing layer mechanical strength is good, to advantages such as medicine disintegrate influence are little, so the employing film coating.
Coating material is selected and bag film-coat technical study:
Finish (increasing weight 3% behind the coating) by Shanghai Colorcon Coating Technology Co., Ltd, 0.5+0.5 * 3%=0.515, so specification is decided to be: the 0.52g/ sheet.
2.6 technology is determined
The logical finished granule Quercetin rate of transform of nephrolith and the medicinal tablet finished product Quercetin rate of transform of the present invention be (seeing Table 15) relatively.
The logical finished granule Quercetin rate of transform of table 15 nephrolith and the medicinal tablet finished product Quercetin rate of transform of the present invention are relatively
Annotate:
By table 15 as seen, the medicinal tablet finished product Quercetin rate of transform of the present invention illustrates that medicinal tablet Study on Forming result of the present invention is reasonable, feasible process a little more than logical granule (sugared type is arranged) the finished product Quercetin rate of transform of nephrolith.Therefore, adopt the decocting technology connecting shaping technical study result of the logical granule long-term production of nephrolith, final determine that medicinal tablet production technology of the present invention is: ten flavors in the prescription, Spora Lygodii, Semen Vaccariae are packed in the cloth bag, decoct with water secondary with eight flavors such as all the other Herba Lysimachiaes, 2.5 hours for the first time, 1.5 hours for the second time, collecting decoction filtered, decompression (75 ℃ ,-0.07Mpa) be concentrated into the extractum that relative density is 1.20～1.25 (75～80 ℃); Make adjuvant with 315g starch, mixing is granulated, dry below 80 ℃; Add 10g carboxymethyl starch sodium and 2.5g magnesium stearate, mixing is pressed into 1000, the bag film-coat, promptly.
Embodiment 7 medicinal tablets of the present invention and the contrast of former granule:
One, dosage form contrast
Medicinal tablet prescription of the present invention derives from the 02nd contained kind of " Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation " SHENSHITONG CHONGJI (granule) (WS
3-B-0304-90) ", for Xuhua Pharmaceutical Co., Ltd., Sichuan changes the exclusive new drug that agent forms on the logical particulate basis of the original nephrolith of company.Function cures mainly: clearing away heat-damp and promoting diuresis, promoting blood circulation and stopping pain, fossil, calculus.Be used for renal calculus, pyelolithiasis, vesical calculus, ureteral calculus.This pharmaceutically dosage form is a tablet, leads on the granule comparison dosage form with former dosage form nephrolith to have a clear superiority in.
" medicinal tablet of the present invention " compares with " nephrolith leads to granule " dosage form
The logical granule of medicinal tablet of the present invention and nephrolith compares: directly oral, do not need warm boiled water, and take more convenient; Directly oral, part is covered the preparation astringent taste, more helps the patient and takes; Obey into dose day and be reduced to by former dosage form day clothes patent medicine 30g and tablet day obey into dose 4.16g, day obeying into dose obviously reduces.Simultaneously tablet also have stability good, carry, characteristics such as storage, convenient transportation, therefore, and have a clear superiority on the logical granule comparison medicinal tablet dosage form of the present invention of former dosage form nephrolith.
Two, technology contrast
Medicinal tablet of the present invention is consistent with the logical granule extraction process of nephrolith, by Study on Forming, reduces supplementary product consumption, has made Tabules, compares with the logical granule of former nephrolith, and the technology of medicine of the present invention is more reasonable.
" medicinal tablet of the present invention " compares with " nephrolith leads to granule " technology
Medicinal tablet of the present invention compares with the logical granule of nephrolith: extraction process is consistent, by Study on Forming, reduces supplementary product consumption, has made Tabules.Add the adjuvant aspect and study the minimizing supplementary product consumption by experiment, make day obey into dose and obviously reduce, be suitable for the crowd because of using Icing Sugar to enlarge patent medicine simultaneously; After moulding process is made tablet by Study on Forming, have a clear superiority on the dosage form with on the logical granule comparison dosage form of former dosage form nephrolith.Therefore, more reasonable with the technology of the logical granule comparison of former nephrolith medicinal tablet of the present invention.
Three, quality standard contrast
Medicinal tablet of the present invention is differentiated and the assay project by increasing thin layer on the basis of the logical granular mass standard of nephrolith, has improved quality standard significantly, makes the quality of the pharmaceutical preparations have more controllability, and the end product quality that dispatches from the factory is more stable.
" medicinal tablet of the present invention " compares with " nephrolith leads to granule " quality standard
The logical granular mass standard of former nephrolith does not have thin layer and differentiates and the assay project, medicinal tablet of the present invention increases Endothelium Corneum Gigeriae Galli, Rhizoma Corydalis, the discriminating of Radix Salviae Miltiorrhizae thin layer and quercetin content by methodological study and measures, improved quality standard significantly, make the quality of the pharmaceutical preparations have more controllability, the end product quality that dispatches from the factory is more stable.
Four, dose contrast
After medicinal tablet of the present invention is made tablet, obeying under the identical situation of crude drug amount with logical granule day of nephrolith, medicinal tablet day of the present invention obeys into dose and obviously reduces, and is about former nephrolith logical particulate 1/7.2.
" medicinal tablet of the present invention " compares with " nephrolith leads to granule " dose
Logical granule day of former nephrolith obeys the crude drug amount and is: 15.3g, and day obeys into dose and is: 30g; Medicinal tablet day of the present invention is obeyed the crude drug amount: 15.3g, day obeys into dose and is: 4.16g.Obeying under the identical situation of crude drug amount with logical granule day of nephrolith, medicinal tablet day of the present invention obeys into dose and obviously reduces, and is about former nephrolith logical particulate 1/7.2.
Claims (10)
1, a kind of pharmaceutical composition with fossil, calculus effect is characterized in that, it is the tablet of being made by following weight percentages and pharmaceutic adjuvant,
Herbal raw material:
Herba Lysimachiae 15.5-17.5%, Semen Vaccariae (parched) 15.5-17.5%, Herba Polygoni Avicularis 9.5-11.5%, Rhizoma Corydalis (processed with vinegar) 4.5-5.5%, boiling hot Endothelium Corneum Gigeriae Galli 5.5-7.5%, Radix Salviae Miltiorrhizae 5.5-7.5%, Radix Aucklandiae 2.5-3.5%, Herba Dianthi 8-10%, Radix Achyranthis Bidentatae 4.5-5.5%, Spora Lygodii 5.5-7.5%;
Pharmaceutic adjuvant:
Filler 14-15% lubricant 0.01-0.15%, disintegrating agent 0.35-0.45%.
2, the pharmaceutical composition with fossil, calculus effect according to claim 1 is characterized in that, described filler is a starch; Lubricant is a magnesium stearate; Disintegrating agent is a carboxymethyl starch sodium.
3, the pharmaceutical composition with fossil, calculus effect according to claim 2 is characterized in that, it is the tablet of being made by following weight percentages and pharmaceutic adjuvant,
Herbal raw material:
Herba Lysimachiae 16.7% Semen Vaccariae (parched) 16.7% Herba Polygoni Avicularis 10.0%
Rhizoma Corydalis (processed with vinegar) 5.0% scalds Endothelium Corneum Gigeriae Galli 6.7% Radix Salviae Miltiorrhizae 6.7%
The Radix Aucklandiae 3.3% Herba Dianthi 8.4% Radix Achyranthis Bidentatae 5.0%
Spora Lygodii 6.7%
Pharmaceutic adjuvant:
Starch 14.1% magnesium stearate 0.1% carboxymethyl starch sodium 0.4%.
According to each described pharmaceutical composition of claim 1-3, it is characterized in that 4, every contains Herba Lysimachiae, Herba Polygoni Avicularis with Quercetin C in the described tablet
15O
10H
7Meter must not be less than 0.10 milligram.
5, a kind of method for preparing each described pharmaceutical composition of claim 1-4, it is characterized in that, in the described 10 flavor herbal raw materials, get Spora Lygodii, Semen Vaccariae and pack in the cloth bag, decoct with water secondary with eight flavors such as all the other Herba Lysimachiaes, 2.5 hours for the first time, 1.5 hours for the second time, collecting decoction, filter, at 75 ℃, be evaporated to relative density under the-0.07Mpa condition and be 1.20～1.25,75～80 ℃ extractum; Make adjuvant with starch, mixing is granulated, dry below 80 ℃; Granulate adds carboxymethyl starch sodium and magnesium stearate, mixing, and compacting is wrapped film-coat in flakes, promptly gets tablet.
6, preparation method according to claim 5 is characterized in that: the consumption of described starch is that the extractum amount is in 1.8～2.1 times of dried cream.
7, preparation method according to claim 6 is characterized in that: the consumption of described starch is that the extractum amount is in 1.85 times of dried cream.
8, preparation method according to claim 5 is characterized in that: the consumption of described carboxymethyl starch sodium is that the extractum amount is in dried cream 2%w/w; The consumption of described magnesium stearate is that the extractum amount is in dried cream 0.5%w/w.
9, preparation method according to claim 5 is characterized in that: the adding method of described carboxymethyl starch sodium, magnesium stearate is the equivalent incremental method, adds carboxymethyl starch sodium earlier, adds magnesium stearate again.
10, preparation method according to claim 5 is characterized in that: wherein said method of granulating is for adopting boiling granulating machine fluidized granulating, and technical parameter is: feed liquor speed 50～55ml/min; Atomisation pressure 0.15Mpa; 55～60 ℃ of temperature of charge; 80～100 ℃ of inlet temperature; 60～65 ℃ of leaving air temps.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102133272A (en) * | 2011-03-24 | 2011-07-27 | 江苏苏南药业实业有限公司 | Preparation method of granules for treating nephrolith |
| CN102716196A (en) * | 2012-07-07 | 2012-10-10 | 广州汉方现代中药研究开发有限公司 | Preparation method for sugarless Shenshitong granule |
| CN105998285A (en) * | 2016-06-12 | 2016-10-12 | 莫佳 | Traditional Chinese medicine preparation for treating urinary calculi and preparation method thereof |
-
2009
- 2009-02-18 CN CN2009100583678A patent/CN101485736B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102133272A (en) * | 2011-03-24 | 2011-07-27 | 江苏苏南药业实业有限公司 | Preparation method of granules for treating nephrolith |
| CN102133272B (en) * | 2011-03-24 | 2012-12-26 | 江苏苏南药业实业有限公司 | Preparation method of granules for treating nephrolith |
| CN102716196A (en) * | 2012-07-07 | 2012-10-10 | 广州汉方现代中药研究开发有限公司 | Preparation method for sugarless Shenshitong granule |
| CN105998285A (en) * | 2016-06-12 | 2016-10-12 | 莫佳 | Traditional Chinese medicine preparation for treating urinary calculi and preparation method thereof |
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| Publication number | Publication date |
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| CN101485736B (en) | 2010-10-20 |
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